HRID1494388

反应详情

EQUATION

反应方程式

HRID 1494388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To one liter of acetone were added 50.0 g (0.31 mol) of 1,4-dihydroxynaphthalene. To the resulting solution then were added 95.0 g (0.69 mol) of powdered potassium carbonate and 65 ml (0.69 mol) of dimethyl sulfate. The resulting mixture was stirred at reflux for 18 hours after which it was diluted with two liters of water and then extracted with methylene chloride. The organic extracts were combined,.dried over sodium sulfate, and evaporated in vacuo to give a black oil. The oil was distilled in vacuo to give 12.5 g of 1,4-dimethoxynaphthalene as an orange crystalline solid. b.p. 155° C. at 5 mm Hg.

WORKUP

后处理

  1. temperatureat reflux for 18 hours after which it
  2. extractionextracted with methylene chloride
  3. customevaporated in vacuo
  4. customto give a black oil
  5. distillationThe oil was distilled in vacuo